Patent
US 9,550,679A Preparation Method of Graphene and Graphene Oxide Based on Mixed Acid System
Linde ZHANG
US
Copyright © 2026 Matter42. All rights reserved.
Claims define the patent's legal scope. Independent claims stand alone; dependent claims (nested) narrow them. Click a claim to expand its dependents.
(C ur rently Amended) A method of preparing graphe n e oxide based on mixed acid system, comprising: a. a preparation of graphite powder: puffing washing drying. and grinding raw mnaterial[[s]] of graphite;_ into processes of washing, drying and grinding, and then putting them sieving the ground graphite througrh a 200-mesh sieve[[s]] to obtain graphite powder; and wherein the raw mnaterial[[s]] of graphite mentioned above are is crystalline flake graphite; b. a preparation of auspension liquid of a&first acid system: mixing the graphite powder obtained from SVG 15106842.10-24-2016.IUQVGFYLPXXIFW1.CLM.1.15.1248.1712.1320.1748.svg 0.12 0.24 Chemistry Black and white a with a intercalator[[,]] to obtain a first mixture: and putting it through conducting an ultrasonic process on the first mixture; wherein said intercalator is the a first acid comiposition[[,]]; and we can obtain graphite the first acid composition providing a first dispersion dispersant including the graphite and a first acid conmositon. with the a mass concentration of the graphite being 0.1 -1 g/mL: wherein said first acid composition includes comprises at least one acid selected from the group consisting of organic strong acid and inorganic strong acid: and puffing the graphite the first acid composition dlispersant through conducting an ultrasonic stirmig process on the first dispersion for 0.5-3 hours, and obtaining to obtain the first acid system: e. a preparation of a& second a ec id system: grinding the a oxidant; Page 42 of 49 Application Serial No, 15/106.842 Applicant: SJJENZHEN CANTONNE TLENERGY SE RVICES CO. -L TD. Art Unit: 1 SVG 15106842.10-24-2016.IUQVGFYLPXXIFW1.CLM.2.2.1941.298.2004.330.svg 0.107 0.21 Chemistry Black and white Response to O ffic e Action ai/ed on 09 SVG 15106842.10-24-2016.IUQVGFYLPXXIFW1.CLM.2.3.1075.354.1121.386.svg 0.107 0.153 Chemistry Black and white 2016 and-add-it solving the around oxidant into the a second acid composition te-dissolve-it-wit at a temperature of being 40-60 o C and-obtainiog-exidant-the cec-on4-aid-comnposition to obtain a first solution with the a mass concentration of the oxidant of bcing 0 SVG 15106842.10-24-2016.IUQVGFYLPXXIFW1.CLM.2.6.1636.614.1720.656.svg 0.14 0.28 Chemistry Black and white/ml: wherein the second acid composition mentioeod abe is either an organic weak acid, or an inorganic weak acid. or a mixture thereof e-f-we-er-mre-f-he~n: adding a long-chain organic acid into the oxidant the cocond acid composition first solution to obtain a second solution; wherein the a mass ratio of ffhe graphite powder obtained hrm step a to the long-chain organic acid is 100:0.1-SVG 15106842.10-24-2016.IUQVGFYLPXXIFW1.CLM.2.11.1100.1074.1128.1109.svg 0.117 0.093 Chemistry Black and white wherein the long-chain organic acid mentioned above is a saturated organic acid with more carbon atoms more than C₁ 0: putting the oxidant thc second acid composition solution with long chain organic acid through conducting an ultrasonic treatment on the second solution ±br 0.5 hours; and naturally cooling the second solution obtaining thc solution of to obtain the second acid system after a process of natural cooling; d. a preparation of a graphene oxide: adding the solution of the first acid system into the second acid system drop by drop with the vclo city being- a rate of 1-2 drops per second to obtain a second mixture mixed liquid; wherein a the volume of the first acid system added to the second acid system is calculated according to the following cquation a first fonnula: SVG 15106842.10-24-2016.IUQVGFYLPXXIFW1.CLM.2.22.962.2120.1430.2180.svg 0.20 1.56 Chemistry Black and white = 1: 2-8 S SVG 15106842.10-24-2016.IUQVGFYLPXXIFW1.CLM.2.23.968.2194.1422.2244.svg 0.167 1.513 Chemistry Black and white wherein C,,, is the mass concentration of the graphite in graphite-the first acid comp osition the first dispersant dispersion, wherein SVG 15106842.10-24-2016.IUQVGFYLPXXIFW1.CLM.2.24.1341.2428.1596.2472.svg 0.147 0.85 Chemistry Black and white ~~ represents the vo lum e of the first acid system, wherein C e represents the mass concentration of oxidant in oxidant the second acid composition the first solution, and wherein VZ SVG 15106842.10-24-2016.IUQVGFYLPXXIFW1.CLM.2.26.1473.2634.1696.2653.svg 0.063 0.743 Chemistry Black and white represents the a volume of the second acid system into which we add the first acid system is added: putting the mixed liquid into conductin the ultrasonic stirring process on the second mmxture for 0.5-3 hours, and; dissolvin g i the second mnixture into water drop by drop with SVG 15106842.10-24-2016.IUQVGFYLPXXIFW1.CLM.2.30.1592.3014.1686.3052.svg 0.127 0.313 Chemistry Black and white enviro nm ent temperature Page 43 of 49 Application Serial No, 15/106,842 Applicant: SJJENZHEN CANTONE TLENERGY SE RVICES CO- LTD. Art Unit: 1 76 Response to O ffic e Action ai/ed on 09 SVG 15106842.10-24-2016.IUQVGFYLPXXIFW1.CLM.3.3.1075.354.1121.386.svg 0.107 0.153 Chemistry Black and white 2016 beig of 70-100 C; plaeing keeping the nii-twe second mixture still for 3-10 min to obtain a eembination combined hquid wherein the a volume of water is calculated according to a_ second formula the fellkwin-equatien: SVG 15106842.10-24-2016.IUQVGFYLPXXIFW1.CLM.3.8.952.858.1432.922.svg 0.213 1.60 Chemistry Black and white 1:20 -50 SVG 15106842.10-24-2016.IUQVGFYLPXXIFW1.CLM.3.11.1061.944.1186.980.svg 0.12 0.417 Chemistry Black and white 'rzs fi r a r i s M-i 2 wh erei n C,,, is the mass concentration of the graphite in graphite the first acid composition the first dispersant dispersion, wherein P, SVG 15106842.10-24-2016.IUQVGFYLPXXIFW1.CLM.3.12.1462.1188.1596.1208.svg 0.067 0.447 Chemistry Black and white represents the volume of the first acid system, wherein P -r represents the a density of water, and wherein represents the vohume of water; treating the combination liquid with conducting the ultrasonic stirring process on the combined liquid for 0.5-3 hours[[j]] then putting it into conducting a centrifuging centrifugal process on the combined liquid at a rate o f with rotating speed being 4000rm'in for 5min and take the to obtain a supernatant: addi ng an ammonium sulfate solution with a mass concentration of being 2-5% into the supernatant to obtain a third solution and salt it out; salting out the third solution to obtain a fourth solution suction filtrate filtrating the fourth solution and wash the to obtain a filter cake; washing the filter cake with deionized water: alcohol washina the filter cake: and diying the filter cake to obtain the obtaining graphene oxide after a process of alcohol washing and drying.
(Curr ently Am ended) The method of claim 1, wherein said first acid composition in step b compri s eo includes at least one acid selected from the group consisting of concentrated sulfiric acid, fiming sulfuric acid, concentrated nitrite acid nitric acid. fuming nitrite acid nitric acid. perchloric acid, chlorosulfonic acid, trifluoroacetic acid (T FA) and sulphaimic acid: and Page 44 of 49 Application Serial No, 15/406,842 Applicant: SHENZHEAN CANTONE TLENERGY SE RVICES CO- LTD. Art Unit: 1 76 Response to O ffic e Action ma i/ed on 09 SVG 15106842.10-24-2016.IUQVGFYLPXXIFW1.CLM.4.3.1075.354.1121.386.svg 0.107 0.153 Chemistry Black and white 2016 wherein said oxidant in-sep-e oipri e includes at least one oxidant selected fiom the group consisting of nitrate. dichromate., persulphate. permanganate. peroxide, phosphorus oxide, and oxy'iodide.
The method of claim 1, wherein said second acid composition. step e comprises includes at least one agent selected from the group consisting of strong phosphoric acid, pyrophosphoric acid, metaphosphoric acid, glacial acetic acid. propionic acid, adipic acid, and g lutaric acid: and wh ere in said lo ng -chain organi c acid mentioned in step e comprices and at least one agent selected from the group consisting of capric acid, undecylenie acid, lauric acid, tetradecanoic acid, palmitic acid. and octadecanioic acid. i (Cur rently A mended) The method of claim 4, w here in said second acid composition i i n step e comprise; includes at least one agent selected from the group consisting of phosphoric acid, glacial acetic acid, and adipie acid; and wherein said long-chain organic acid in step c comprises includes at least one agent selected from the group consisting of capric acid. palmitic acid, and octadecanioic acid.
(C urr ently Amended) [[A]] The method for preparing graphene of claim 1, further comprising: e. putting adding the graphene oxide obtained according to claim I into a dispersant with a high boiling point, and putting it through conducing an ultrasonic distribution treatment to obtain a j graphene oxide dispersant second dispersion with a concentration of 0.1-1 g/ml: f. putting adding a reducing agent into the second dispersio n; graphene oxide dispersant obtained from ctop e wherein the reducing agent is one of organic acid and organic acid salt, or a mixture of two or more f organic acids and organic acid salts: wherein the a mass ratio of the graphene oxide graphene oxide dispersant to the reducing agent is 1: 2-8; Page 45 of 49 Application Serial No, 15/406,842 Applicant: SHENZHEAN CANTONE TLENERGY SE RVICES CO- LTD. Art Unit: 1 76 Response to Offic e Action mailed on 09 SVG 15106842.10-24-2016.IUQVGFYLPXXIFW1.CLM.5.3.1075.354.1121.386.svg 0.107 0.153 Chemistry Black and white/2016 putting the graphene-ex-ide-depersant with-the-reduemg-agent obtained-rem-sep-f-t-e SVG 15106842.10-24-2016.IUQVGFYLPXXIFW1.CLM.5.4.378.476.400.508.svg 0.107 0.073 Chemistry Black and white conducting a microwave heating process on the second dispersion at of 400-900W for 5-30min; pttA-he-g phenet-eide--ite conducting the ultrasonic stripping process on the second dispersion at 4 100-600W for 0,5-3 hours: and h. add ina water into the second dispersion fifth solutio n-gaphene-e-ie4spersant obtemed in stop g, and wherein a the volume of the water is the same as that of the second dispersion the dispersant: obtaining graphene after filtering suction filtrating. washing, and drying the fifth solution to obtain the graphene composition of water and the graphene oxide dispersant by suction filtrate, and washing and drying.
(C urr ently Am ended) The method of clai m 6, wherein said reducing a g ent in step f comprises i ncludes at least one agent selected from the group consisting of citric acid, gluconic acid, formic acid, ascorbic acid, oxalic acid, sodium citrate, sodimn gluconate, sodium formate, sodium ascorbate, and sodium oxalate.
(C urr ently Amended) The method of claim 9. wherein said reducing agent in step f comprises includes at least one agent selected from the group consisting of oxalic acid, sodium citrate. fonuic acid, and sodium formnate, or a mixture of two or more of them. Page 46 of 49
Materials described outside the worked examples.
crystalline flake graphite
graphene oxide
graphene
ammonium sulfate
(NH₄)2SO₄
first acid composition (strong acid intercalator)
oxidant (nitrate, dichromate, persulphate, permanganate, peroxide, phosphorus oxide, oxyiodide)
first acid composition (concentrated sulfuric acid, fuming nitric acid, perchloric acid, chlorosulfonic acid)
oxidant (nitrate, potassium permanganate, ammonium persulfate, potassium persulfate, nitrite of potash, phosphorus pentoxide, iodine pentoxide)
second acid composition (phosphoric acid, pyrophosphoric acid, metaphosphoric acid, glacial acetic acid, propionic acid, adipic acid, glutaric acid)
long-chain organic acid (capric acid, undecylenic acid, lauric acid, tetradecanoic acid, palmitic acid, octadecanoic acid)
reducing agent (organic acid or organic acid salt)
high boiling point dispersant (phosphoric acid 80%, phosphoric acid 85%, glycerol, glycol, N-methyl-pyrrolidone, triethylene glycol, cyclohexanol)
high boiling point dispersant (phosphoric acid 80%, glycerol, N-methyl-pyrrolidone)
reducing agent (citric acid, gluconic acid, formic acid, ascorbic acid, oxalic acid, sodium citrate, sodium gluconate, sodium formate, sodium ascorbate, sodium oxalate)
reducing agent (oxalic acid, sodium citrate, formic acid, sodium formate)
Additional fabrication and treatment steps described in the patent.
Performance values and ranges asserted in the specification or claims.
| Property | Value | Material |
|---|---|---|
Temperature | ≤ 40 °C | — |
Duration | 0.5–3 hours | — |
Duration | 3–10 min | — |
— | 400–900 W | — |
Duration | 5–30 min | — |
— | 100–600 W | — |
Duration | 5-3 hours | — |
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Claims define the patent's legal scope. Independent claims stand alone; dependent claims (nested) narrow them. Click a claim to expand its dependents.
(C ur rently Amended) A method of preparing graphe n e oxide based on mixed acid system, comprising: a. a preparation of graphite powder: puffing washing drying. and grinding raw mnaterial[[s]] of graphite;_ into processes of washing, drying and grinding, and then putting them sieving the ground graphite througrh a 200-mesh sieve[[s]] to obtain graphite powder; and wherein the raw mnaterial[[s]] of graphite mentioned above are is crystalline flake graphite; b. a preparation of auspension liquid of a&first acid system: mixing the graphite powder obtained from SVG 15106842.10-24-2016.IUQVGFYLPXXIFW1.CLM.1.15.1248.1712.1320.1748.svg 0.12 0.24 Chemistry Black and white a with a intercalator[[,]] to obtain a first mixture: and putting it through conducting an ultrasonic process on the first mixture; wherein said intercalator is the a first acid comiposition[[,]]; and we can obtain graphite the first acid composition providing a first dispersion dispersant including the graphite and a first acid conmositon. with the a mass concentration of the graphite being 0.1 -1 g/mL: wherein said first acid composition includes comprises at least one acid selected from the group consisting of organic strong acid and inorganic strong acid: and puffing the graphite the first acid composition dlispersant through conducting an ultrasonic stirmig process on the first dispersion for 0.5-3 hours, and obtaining to obtain the first acid system: e. a preparation of a& second a ec id system: grinding the a oxidant; Page 42 of 49 Application Serial No, 15/106.842 Applicant: SJJENZHEN CANTONNE TLENERGY SE RVICES CO. -L TD. Art Unit: 1 SVG 15106842.10-24-2016.IUQVGFYLPXXIFW1.CLM.2.2.1941.298.2004.330.svg 0.107 0.21 Chemistry Black and white Response to O ffic e Action ai/ed on 09 SVG 15106842.10-24-2016.IUQVGFYLPXXIFW1.CLM.2.3.1075.354.1121.386.svg 0.107 0.153 Chemistry Black and white 2016 and-add-it solving the around oxidant into the a second acid composition te-dissolve-it-wit at a temperature of being 40-60 o C and-obtainiog-exidant-the cec-on4-aid-comnposition to obtain a first solution with the a mass concentration of the oxidant of bcing 0 SVG 15106842.10-24-2016.IUQVGFYLPXXIFW1.CLM.2.6.1636.614.1720.656.svg 0.14 0.28 Chemistry Black and white/ml: wherein the second acid composition mentioeod abe is either an organic weak acid, or an inorganic weak acid. or a mixture thereof e-f-we-er-mre-f-he~n: adding a long-chain organic acid into the oxidant the cocond acid composition first solution to obtain a second solution; wherein the a mass ratio of ffhe graphite powder obtained hrm step a to the long-chain organic acid is 100:0.1-SVG 15106842.10-24-2016.IUQVGFYLPXXIFW1.CLM.2.11.1100.1074.1128.1109.svg 0.117 0.093 Chemistry Black and white wherein the long-chain organic acid mentioned above is a saturated organic acid with more carbon atoms more than C₁ 0: putting the oxidant thc second acid composition solution with long chain organic acid through conducting an ultrasonic treatment on the second solution ±br 0.5 hours; and naturally cooling the second solution obtaining thc solution of to obtain the second acid system after a process of natural cooling; d. a preparation of a graphene oxide: adding the solution of the first acid system into the second acid system drop by drop with the vclo city being- a rate of 1-2 drops per second to obtain a second mixture mixed liquid; wherein a the volume of the first acid system added to the second acid system is calculated according to the following cquation a first fonnula: SVG 15106842.10-24-2016.IUQVGFYLPXXIFW1.CLM.2.22.962.2120.1430.2180.svg 0.20 1.56 Chemistry Black and white = 1: 2-8 S SVG 15106842.10-24-2016.IUQVGFYLPXXIFW1.CLM.2.23.968.2194.1422.2244.svg 0.167 1.513 Chemistry Black and white wherein C,,, is the mass concentration of the graphite in graphite-the first acid comp osition the first dispersant dispersion, wherein SVG 15106842.10-24-2016.IUQVGFYLPXXIFW1.CLM.2.24.1341.2428.1596.2472.svg 0.147 0.85 Chemistry Black and white ~~ represents the vo lum e of the first acid system, wherein C e represents the mass concentration of oxidant in oxidant the second acid composition the first solution, and wherein VZ SVG 15106842.10-24-2016.IUQVGFYLPXXIFW1.CLM.2.26.1473.2634.1696.2653.svg 0.063 0.743 Chemistry Black and white represents the a volume of the second acid system into which we add the first acid system is added: putting the mixed liquid into conductin the ultrasonic stirring process on the second mmxture for 0.5-3 hours, and; dissolvin g i the second mnixture into water drop by drop with SVG 15106842.10-24-2016.IUQVGFYLPXXIFW1.CLM.2.30.1592.3014.1686.3052.svg 0.127 0.313 Chemistry Black and white enviro nm ent temperature Page 43 of 49 Application Serial No, 15/106,842 Applicant: SJJENZHEN CANTONE TLENERGY SE RVICES CO- LTD. Art Unit: 1 76 Response to O ffic e Action ai/ed on 09 SVG 15106842.10-24-2016.IUQVGFYLPXXIFW1.CLM.3.3.1075.354.1121.386.svg 0.107 0.153 Chemistry Black and white 2016 beig of 70-100 C; plaeing keeping the nii-twe second mixture still for 3-10 min to obtain a eembination combined hquid wherein the a volume of water is calculated according to a_ second formula the fellkwin-equatien: SVG 15106842.10-24-2016.IUQVGFYLPXXIFW1.CLM.3.8.952.858.1432.922.svg 0.213 1.60 Chemistry Black and white 1:20 -50 SVG 15106842.10-24-2016.IUQVGFYLPXXIFW1.CLM.3.11.1061.944.1186.980.svg 0.12 0.417 Chemistry Black and white 'rzs fi r a r i s M-i 2 wh erei n C,,, is the mass concentration of the graphite in graphite the first acid composition the first dispersant dispersion, wherein P, SVG 15106842.10-24-2016.IUQVGFYLPXXIFW1.CLM.3.12.1462.1188.1596.1208.svg 0.067 0.447 Chemistry Black and white represents the volume of the first acid system, wherein P -r represents the a density of water, and wherein represents the vohume of water; treating the combination liquid with conducting the ultrasonic stirring process on the combined liquid for 0.5-3 hours[[j]] then putting it into conducting a centrifuging centrifugal process on the combined liquid at a rate o f with rotating speed being 4000rm'in for 5min and take the to obtain a supernatant: addi ng an ammonium sulfate solution with a mass concentration of being 2-5% into the supernatant to obtain a third solution and salt it out; salting out the third solution to obtain a fourth solution suction filtrate filtrating the fourth solution and wash the to obtain a filter cake; washing the filter cake with deionized water: alcohol washina the filter cake: and diying the filter cake to obtain the obtaining graphene oxide after a process of alcohol washing and drying.
(Curr ently Am ended) The method of claim 1, wherein said first acid composition in step b compri s eo includes at least one acid selected from the group consisting of concentrated sulfiric acid, fiming sulfuric acid, concentrated nitrite acid nitric acid. fuming nitrite acid nitric acid. perchloric acid, chlorosulfonic acid, trifluoroacetic acid (T FA) and sulphaimic acid: and Page 44 of 49 Application Serial No, 15/406,842 Applicant: SHENZHEAN CANTONE TLENERGY SE RVICES CO- LTD. Art Unit: 1 76 Response to O ffic e Action ma i/ed on 09 SVG 15106842.10-24-2016.IUQVGFYLPXXIFW1.CLM.4.3.1075.354.1121.386.svg 0.107 0.153 Chemistry Black and white 2016 wherein said oxidant in-sep-e oipri e includes at least one oxidant selected fiom the group consisting of nitrate. dichromate., persulphate. permanganate. peroxide, phosphorus oxide, and oxy'iodide.
The method of claim 1, wherein said second acid composition. step e comprises includes at least one agent selected from the group consisting of strong phosphoric acid, pyrophosphoric acid, metaphosphoric acid, glacial acetic acid. propionic acid, adipic acid, and g lutaric acid: and wh ere in said lo ng -chain organi c acid mentioned in step e comprices and at least one agent selected from the group consisting of capric acid, undecylenie acid, lauric acid, tetradecanoic acid, palmitic acid. and octadecanioic acid. i (Cur rently A mended) The method of claim 4, w here in said second acid composition i i n step e comprise; includes at least one agent selected from the group consisting of phosphoric acid, glacial acetic acid, and adipie acid; and wherein said long-chain organic acid in step c comprises includes at least one agent selected from the group consisting of capric acid. palmitic acid, and octadecanioic acid.
(C urr ently Amended) [[A]] The method for preparing graphene of claim 1, further comprising: e. putting adding the graphene oxide obtained according to claim I into a dispersant with a high boiling point, and putting it through conducing an ultrasonic distribution treatment to obtain a j graphene oxide dispersant second dispersion with a concentration of 0.1-1 g/ml: f. putting adding a reducing agent into the second dispersio n; graphene oxide dispersant obtained from ctop e wherein the reducing agent is one of organic acid and organic acid salt, or a mixture of two or more f organic acids and organic acid salts: wherein the a mass ratio of the graphene oxide graphene oxide dispersant to the reducing agent is 1: 2-8; Page 45 of 49 Application Serial No, 15/406,842 Applicant: SHENZHEAN CANTONE TLENERGY SE RVICES CO- LTD. Art Unit: 1 76 Response to Offic e Action mailed on 09 SVG 15106842.10-24-2016.IUQVGFYLPXXIFW1.CLM.5.3.1075.354.1121.386.svg 0.107 0.153 Chemistry Black and white/2016 putting the graphene-ex-ide-depersant with-the-reduemg-agent obtained-rem-sep-f-t-e SVG 15106842.10-24-2016.IUQVGFYLPXXIFW1.CLM.5.4.378.476.400.508.svg 0.107 0.073 Chemistry Black and white conducting a microwave heating process on the second dispersion at of 400-900W for 5-30min; pttA-he-g phenet-eide--ite conducting the ultrasonic stripping process on the second dispersion at 4 100-600W for 0,5-3 hours: and h. add ina water into the second dispersion fifth solutio n-gaphene-e-ie4spersant obtemed in stop g, and wherein a the volume of the water is the same as that of the second dispersion the dispersant: obtaining graphene after filtering suction filtrating. washing, and drying the fifth solution to obtain the graphene composition of water and the graphene oxide dispersant by suction filtrate, and washing and drying.
(C urr ently Am ended) The method of clai m 6, wherein said reducing a g ent in step f comprises i ncludes at least one agent selected from the group consisting of citric acid, gluconic acid, formic acid, ascorbic acid, oxalic acid, sodium citrate, sodimn gluconate, sodium formate, sodium ascorbate, and sodium oxalate.
(C urr ently Amended) The method of claim 9. wherein said reducing agent in step f comprises includes at least one agent selected from the group consisting of oxalic acid, sodium citrate. fonuic acid, and sodium formnate, or a mixture of two or more of them. Page 46 of 49
Materials described outside the worked examples.
crystalline flake graphite
graphene oxide
graphene
ammonium sulfate
(NH₄)2SO₄
first acid composition (strong acid intercalator)
oxidant (nitrate, dichromate, persulphate, permanganate, peroxide, phosphorus oxide, oxyiodide)
first acid composition (concentrated sulfuric acid, fuming nitric acid, perchloric acid, chlorosulfonic acid)
oxidant (nitrate, potassium permanganate, ammonium persulfate, potassium persulfate, nitrite of potash, phosphorus pentoxide, iodine pentoxide)
second acid composition (phosphoric acid, pyrophosphoric acid, metaphosphoric acid, glacial acetic acid, propionic acid, adipic acid, glutaric acid)
long-chain organic acid (capric acid, undecylenic acid, lauric acid, tetradecanoic acid, palmitic acid, octadecanoic acid)
reducing agent (organic acid or organic acid salt)
high boiling point dispersant (phosphoric acid 80%, phosphoric acid 85%, glycerol, glycol, N-methyl-pyrrolidone, triethylene glycol, cyclohexanol)
high boiling point dispersant (phosphoric acid 80%, glycerol, N-methyl-pyrrolidone)
reducing agent (citric acid, gluconic acid, formic acid, ascorbic acid, oxalic acid, sodium citrate, sodium gluconate, sodium formate, sodium ascorbate, sodium oxalate)
reducing agent (oxalic acid, sodium citrate, formic acid, sodium formate)
Additional fabrication and treatment steps described in the patent.
Performance values and ranges asserted in the specification or claims.
| Property | Value | Material |
|---|---|---|
Temperature | ≤ 40 °C | — |
Duration | 0.5–3 hours | — |
Duration | 3–10 min | — |
— | 400–900 W | — |
Duration | 5–30 min | — |
— | 100–600 W | — |
Duration | 5-3 hours | — |
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SYSTEM AND METHOD FOR PREPARING GRAPHENE OXIDE AND REDUCED GRAPHENE OXIDE
Claims define the patent's legal scope. Independent claims stand alone; dependent claims (nested) narrow them. Click a claim to expand its dependents.
(C ur rently Amended) A method of preparing graphe n e oxide based on mixed acid system, comprising: a. a preparation of graphite powder: puffing washing drying. and grinding raw mnaterial[[s]] of graphite;_ into processes of washing, drying and grinding, and then putting them sieving the ground graphite througrh a 200-mesh sieve[[s]] to obtain graphite powder; and wherein the raw mnaterial[[s]] of graphite mentioned above are is crystalline flake graphite; b. a preparation of auspension liquid of a&first acid system: mixing the graphite powder obtained from SVG 15106842.10-24-2016.IUQVGFYLPXXIFW1.CLM.1.15.1248.1712.1320.1748.svg 0.12 0.24 Chemistry Black and white a with a intercalator[[,]] to obtain a first mixture: and putting it through conducting an ultrasonic process on the first mixture; wherein said intercalator is the a first acid comiposition[[,]]; and we can obtain graphite the first acid composition providing a first dispersion dispersant including the graphite and a first acid conmositon. with the a mass concentration of the graphite being 0.1 -1 g/mL: wherein said first acid composition includes comprises at least one acid selected from the group consisting of organic strong acid and inorganic strong acid: and puffing the graphite the first acid composition dlispersant through conducting an ultrasonic stirmig process on the first dispersion for 0.5-3 hours, and obtaining to obtain the first acid system: e. a preparation of a& second a ec id system: grinding the a oxidant; Page 42 of 49 Application Serial No, 15/106.842 Applicant: SJJENZHEN CANTONNE TLENERGY SE RVICES CO. -L TD. Art Unit: 1 SVG 15106842.10-24-2016.IUQVGFYLPXXIFW1.CLM.2.2.1941.298.2004.330.svg 0.107 0.21 Chemistry Black and white Response to O ffic e Action ai/ed on 09 SVG 15106842.10-24-2016.IUQVGFYLPXXIFW1.CLM.2.3.1075.354.1121.386.svg 0.107 0.153 Chemistry Black and white 2016 and-add-it solving the around oxidant into the a second acid composition te-dissolve-it-wit at a temperature of being 40-60 o C and-obtainiog-exidant-the cec-on4-aid-comnposition to obtain a first solution with the a mass concentration of the oxidant of bcing 0 SVG 15106842.10-24-2016.IUQVGFYLPXXIFW1.CLM.2.6.1636.614.1720.656.svg 0.14 0.28 Chemistry Black and white/ml: wherein the second acid composition mentioeod abe is either an organic weak acid, or an inorganic weak acid. or a mixture thereof e-f-we-er-mre-f-he~n: adding a long-chain organic acid into the oxidant the cocond acid composition first solution to obtain a second solution; wherein the a mass ratio of ffhe graphite powder obtained hrm step a to the long-chain organic acid is 100:0.1-SVG 15106842.10-24-2016.IUQVGFYLPXXIFW1.CLM.2.11.1100.1074.1128.1109.svg 0.117 0.093 Chemistry Black and white wherein the long-chain organic acid mentioned above is a saturated organic acid with more carbon atoms more than C₁ 0: putting the oxidant thc second acid composition solution with long chain organic acid through conducting an ultrasonic treatment on the second solution ±br 0.5 hours; and naturally cooling the second solution obtaining thc solution of to obtain the second acid system after a process of natural cooling; d. a preparation of a graphene oxide: adding the solution of the first acid system into the second acid system drop by drop with the vclo city being- a rate of 1-2 drops per second to obtain a second mixture mixed liquid; wherein a the volume of the first acid system added to the second acid system is calculated according to the following cquation a first fonnula: SVG 15106842.10-24-2016.IUQVGFYLPXXIFW1.CLM.2.22.962.2120.1430.2180.svg 0.20 1.56 Chemistry Black and white = 1: 2-8 S SVG 15106842.10-24-2016.IUQVGFYLPXXIFW1.CLM.2.23.968.2194.1422.2244.svg 0.167 1.513 Chemistry Black and white wherein C,,, is the mass concentration of the graphite in graphite-the first acid comp osition the first dispersant dispersion, wherein SVG 15106842.10-24-2016.IUQVGFYLPXXIFW1.CLM.2.24.1341.2428.1596.2472.svg 0.147 0.85 Chemistry Black and white ~~ represents the vo lum e of the first acid system, wherein C e represents the mass concentration of oxidant in oxidant the second acid composition the first solution, and wherein VZ SVG 15106842.10-24-2016.IUQVGFYLPXXIFW1.CLM.2.26.1473.2634.1696.2653.svg 0.063 0.743 Chemistry Black and white represents the a volume of the second acid system into which we add the first acid system is added: putting the mixed liquid into conductin the ultrasonic stirring process on the second mmxture for 0.5-3 hours, and; dissolvin g i the second mnixture into water drop by drop with SVG 15106842.10-24-2016.IUQVGFYLPXXIFW1.CLM.2.30.1592.3014.1686.3052.svg 0.127 0.313 Chemistry Black and white enviro nm ent temperature Page 43 of 49 Application Serial No, 15/106,842 Applicant: SJJENZHEN CANTONE TLENERGY SE RVICES CO- LTD. Art Unit: 1 76 Response to O ffic e Action ai/ed on 09 SVG 15106842.10-24-2016.IUQVGFYLPXXIFW1.CLM.3.3.1075.354.1121.386.svg 0.107 0.153 Chemistry Black and white 2016 beig of 70-100 C; plaeing keeping the nii-twe second mixture still for 3-10 min to obtain a eembination combined hquid wherein the a volume of water is calculated according to a_ second formula the fellkwin-equatien: SVG 15106842.10-24-2016.IUQVGFYLPXXIFW1.CLM.3.8.952.858.1432.922.svg 0.213 1.60 Chemistry Black and white 1:20 -50 SVG 15106842.10-24-2016.IUQVGFYLPXXIFW1.CLM.3.11.1061.944.1186.980.svg 0.12 0.417 Chemistry Black and white 'rzs fi r a r i s M-i 2 wh erei n C,,, is the mass concentration of the graphite in graphite the first acid composition the first dispersant dispersion, wherein P, SVG 15106842.10-24-2016.IUQVGFYLPXXIFW1.CLM.3.12.1462.1188.1596.1208.svg 0.067 0.447 Chemistry Black and white represents the volume of the first acid system, wherein P -r represents the a density of water, and wherein represents the vohume of water; treating the combination liquid with conducting the ultrasonic stirring process on the combined liquid for 0.5-3 hours[[j]] then putting it into conducting a centrifuging centrifugal process on the combined liquid at a rate o f with rotating speed being 4000rm'in for 5min and take the to obtain a supernatant: addi ng an ammonium sulfate solution with a mass concentration of being 2-5% into the supernatant to obtain a third solution and salt it out; salting out the third solution to obtain a fourth solution suction filtrate filtrating the fourth solution and wash the to obtain a filter cake; washing the filter cake with deionized water: alcohol washina the filter cake: and diying the filter cake to obtain the obtaining graphene oxide after a process of alcohol washing and drying.
(Curr ently Am ended) The method of claim 1, wherein said first acid composition in step b compri s eo includes at least one acid selected from the group consisting of concentrated sulfiric acid, fiming sulfuric acid, concentrated nitrite acid nitric acid. fuming nitrite acid nitric acid. perchloric acid, chlorosulfonic acid, trifluoroacetic acid (T FA) and sulphaimic acid: and Page 44 of 49 Application Serial No, 15/406,842 Applicant: SHENZHEAN CANTONE TLENERGY SE RVICES CO- LTD. Art Unit: 1 76 Response to O ffic e Action ma i/ed on 09 SVG 15106842.10-24-2016.IUQVGFYLPXXIFW1.CLM.4.3.1075.354.1121.386.svg 0.107 0.153 Chemistry Black and white 2016 wherein said oxidant in-sep-e oipri e includes at least one oxidant selected fiom the group consisting of nitrate. dichromate., persulphate. permanganate. peroxide, phosphorus oxide, and oxy'iodide.
The method of claim 1, wherein said second acid composition. step e comprises includes at least one agent selected from the group consisting of strong phosphoric acid, pyrophosphoric acid, metaphosphoric acid, glacial acetic acid. propionic acid, adipic acid, and g lutaric acid: and wh ere in said lo ng -chain organi c acid mentioned in step e comprices and at least one agent selected from the group consisting of capric acid, undecylenie acid, lauric acid, tetradecanoic acid, palmitic acid. and octadecanioic acid. i (Cur rently A mended) The method of claim 4, w here in said second acid composition i i n step e comprise; includes at least one agent selected from the group consisting of phosphoric acid, glacial acetic acid, and adipie acid; and wherein said long-chain organic acid in step c comprises includes at least one agent selected from the group consisting of capric acid. palmitic acid, and octadecanioic acid.
(C urr ently Amended) [[A]] The method for preparing graphene of claim 1, further comprising: e. putting adding the graphene oxide obtained according to claim I into a dispersant with a high boiling point, and putting it through conducing an ultrasonic distribution treatment to obtain a j graphene oxide dispersant second dispersion with a concentration of 0.1-1 g/ml: f. putting adding a reducing agent into the second dispersio n; graphene oxide dispersant obtained from ctop e wherein the reducing agent is one of organic acid and organic acid salt, or a mixture of two or more f organic acids and organic acid salts: wherein the a mass ratio of the graphene oxide graphene oxide dispersant to the reducing agent is 1: 2-8; Page 45 of 49 Application Serial No, 15/406,842 Applicant: SHENZHEAN CANTONE TLENERGY SE RVICES CO- LTD. Art Unit: 1 76 Response to Offic e Action mailed on 09 SVG 15106842.10-24-2016.IUQVGFYLPXXIFW1.CLM.5.3.1075.354.1121.386.svg 0.107 0.153 Chemistry Black and white/2016 putting the graphene-ex-ide-depersant with-the-reduemg-agent obtained-rem-sep-f-t-e SVG 15106842.10-24-2016.IUQVGFYLPXXIFW1.CLM.5.4.378.476.400.508.svg 0.107 0.073 Chemistry Black and white conducting a microwave heating process on the second dispersion at of 400-900W for 5-30min; pttA-he-g phenet-eide--ite conducting the ultrasonic stripping process on the second dispersion at 4 100-600W for 0,5-3 hours: and h. add ina water into the second dispersion fifth solutio n-gaphene-e-ie4spersant obtemed in stop g, and wherein a the volume of the water is the same as that of the second dispersion the dispersant: obtaining graphene after filtering suction filtrating. washing, and drying the fifth solution to obtain the graphene composition of water and the graphene oxide dispersant by suction filtrate, and washing and drying.
(C urr ently Am ended) The method of clai m 6, wherein said reducing a g ent in step f comprises i ncludes at least one agent selected from the group consisting of citric acid, gluconic acid, formic acid, ascorbic acid, oxalic acid, sodium citrate, sodimn gluconate, sodium formate, sodium ascorbate, and sodium oxalate.
(C urr ently Amended) The method of claim 9. wherein said reducing agent in step f comprises includes at least one agent selected from the group consisting of oxalic acid, sodium citrate. fonuic acid, and sodium formnate, or a mixture of two or more of them. Page 46 of 49
Materials described outside the worked examples.
crystalline flake graphite
graphene oxide
graphene
ammonium sulfate
(NH₄)2SO₄
first acid composition (strong acid intercalator)
oxidant (nitrate, dichromate, persulphate, permanganate, peroxide, phosphorus oxide, oxyiodide)
first acid composition (concentrated sulfuric acid, fuming nitric acid, perchloric acid, chlorosulfonic acid)
oxidant (nitrate, potassium permanganate, ammonium persulfate, potassium persulfate, nitrite of potash, phosphorus pentoxide, iodine pentoxide)
second acid composition (phosphoric acid, pyrophosphoric acid, metaphosphoric acid, glacial acetic acid, propionic acid, adipic acid, glutaric acid)
long-chain organic acid (capric acid, undecylenic acid, lauric acid, tetradecanoic acid, palmitic acid, octadecanoic acid)
reducing agent (organic acid or organic acid salt)
high boiling point dispersant (phosphoric acid 80%, phosphoric acid 85%, glycerol, glycol, N-methyl-pyrrolidone, triethylene glycol, cyclohexanol)
high boiling point dispersant (phosphoric acid 80%, glycerol, N-methyl-pyrrolidone)
reducing agent (citric acid, gluconic acid, formic acid, ascorbic acid, oxalic acid, sodium citrate, sodium gluconate, sodium formate, sodium ascorbate, sodium oxalate)
reducing agent (oxalic acid, sodium citrate, formic acid, sodium formate)
Additional fabrication and treatment steps described in the patent.
Performance values and ranges asserted in the specification or claims.
| Property | Value | Material |
|---|---|---|
Temperature | ≤ 40 °C | — |
Duration | 0.5–3 hours | — |
Duration | 3–10 min | — |
— | 400–900 W | — |
Duration | 5–30 min | — |
— | 100–600 W | — |
Duration | 5-3 hours | — |
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Claims define the patent's legal scope. Independent claims stand alone; dependent claims (nested) narrow them. Click a claim to expand its dependents.
(C ur rently Amended) A method of preparing graphe n e oxide based on mixed acid system, comprising: a. a preparation of graphite powder: puffing washing drying. and grinding raw mnaterial[[s]] of graphite;_ into processes of washing, drying and grinding, and then putting them sieving the ground graphite througrh a 200-mesh sieve[[s]] to obtain graphite powder; and wherein the raw mnaterial[[s]] of graphite mentioned above are is crystalline flake graphite; b. a preparation of auspension liquid of a&first acid system: mixing the graphite powder obtained from SVG 15106842.10-24-2016.IUQVGFYLPXXIFW1.CLM.1.15.1248.1712.1320.1748.svg 0.12 0.24 Chemistry Black and white a with a intercalator[[,]] to obtain a first mixture: and putting it through conducting an ultrasonic process on the first mixture; wherein said intercalator is the a first acid comiposition[[,]]; and we can obtain graphite the first acid composition providing a first dispersion dispersant including the graphite and a first acid conmositon. with the a mass concentration of the graphite being 0.1 -1 g/mL: wherein said first acid composition includes comprises at least one acid selected from the group consisting of organic strong acid and inorganic strong acid: and puffing the graphite the first acid composition dlispersant through conducting an ultrasonic stirmig process on the first dispersion for 0.5-3 hours, and obtaining to obtain the first acid system: e. a preparation of a& second a ec id system: grinding the a oxidant; Page 42 of 49 Application Serial No, 15/106.842 Applicant: SJJENZHEN CANTONNE TLENERGY SE RVICES CO. -L TD. Art Unit: 1 SVG 15106842.10-24-2016.IUQVGFYLPXXIFW1.CLM.2.2.1941.298.2004.330.svg 0.107 0.21 Chemistry Black and white Response to O ffic e Action ai/ed on 09 SVG 15106842.10-24-2016.IUQVGFYLPXXIFW1.CLM.2.3.1075.354.1121.386.svg 0.107 0.153 Chemistry Black and white 2016 and-add-it solving the around oxidant into the a second acid composition te-dissolve-it-wit at a temperature of being 40-60 o C and-obtainiog-exidant-the cec-on4-aid-comnposition to obtain a first solution with the a mass concentration of the oxidant of bcing 0 SVG 15106842.10-24-2016.IUQVGFYLPXXIFW1.CLM.2.6.1636.614.1720.656.svg 0.14 0.28 Chemistry Black and white/ml: wherein the second acid composition mentioeod abe is either an organic weak acid, or an inorganic weak acid. or a mixture thereof e-f-we-er-mre-f-he~n: adding a long-chain organic acid into the oxidant the cocond acid composition first solution to obtain a second solution; wherein the a mass ratio of ffhe graphite powder obtained hrm step a to the long-chain organic acid is 100:0.1-SVG 15106842.10-24-2016.IUQVGFYLPXXIFW1.CLM.2.11.1100.1074.1128.1109.svg 0.117 0.093 Chemistry Black and white wherein the long-chain organic acid mentioned above is a saturated organic acid with more carbon atoms more than C₁ 0: putting the oxidant thc second acid composition solution with long chain organic acid through conducting an ultrasonic treatment on the second solution ±br 0.5 hours; and naturally cooling the second solution obtaining thc solution of to obtain the second acid system after a process of natural cooling; d. a preparation of a graphene oxide: adding the solution of the first acid system into the second acid system drop by drop with the vclo city being- a rate of 1-2 drops per second to obtain a second mixture mixed liquid; wherein a the volume of the first acid system added to the second acid system is calculated according to the following cquation a first fonnula: SVG 15106842.10-24-2016.IUQVGFYLPXXIFW1.CLM.2.22.962.2120.1430.2180.svg 0.20 1.56 Chemistry Black and white = 1: 2-8 S SVG 15106842.10-24-2016.IUQVGFYLPXXIFW1.CLM.2.23.968.2194.1422.2244.svg 0.167 1.513 Chemistry Black and white wherein C,,, is the mass concentration of the graphite in graphite-the first acid comp osition the first dispersant dispersion, wherein SVG 15106842.10-24-2016.IUQVGFYLPXXIFW1.CLM.2.24.1341.2428.1596.2472.svg 0.147 0.85 Chemistry Black and white ~~ represents the vo lum e of the first acid system, wherein C e represents the mass concentration of oxidant in oxidant the second acid composition the first solution, and wherein VZ SVG 15106842.10-24-2016.IUQVGFYLPXXIFW1.CLM.2.26.1473.2634.1696.2653.svg 0.063 0.743 Chemistry Black and white represents the a volume of the second acid system into which we add the first acid system is added: putting the mixed liquid into conductin the ultrasonic stirring process on the second mmxture for 0.5-3 hours, and; dissolvin g i the second mnixture into water drop by drop with SVG 15106842.10-24-2016.IUQVGFYLPXXIFW1.CLM.2.30.1592.3014.1686.3052.svg 0.127 0.313 Chemistry Black and white enviro nm ent temperature Page 43 of 49 Application Serial No, 15/106,842 Applicant: SJJENZHEN CANTONE TLENERGY SE RVICES CO- LTD. Art Unit: 1 76 Response to O ffic e Action ai/ed on 09 SVG 15106842.10-24-2016.IUQVGFYLPXXIFW1.CLM.3.3.1075.354.1121.386.svg 0.107 0.153 Chemistry Black and white 2016 beig of 70-100 C; plaeing keeping the nii-twe second mixture still for 3-10 min to obtain a eembination combined hquid wherein the a volume of water is calculated according to a_ second formula the fellkwin-equatien: SVG 15106842.10-24-2016.IUQVGFYLPXXIFW1.CLM.3.8.952.858.1432.922.svg 0.213 1.60 Chemistry Black and white 1:20 -50 SVG 15106842.10-24-2016.IUQVGFYLPXXIFW1.CLM.3.11.1061.944.1186.980.svg 0.12 0.417 Chemistry Black and white 'rzs fi r a r i s M-i 2 wh erei n C,,, is the mass concentration of the graphite in graphite the first acid composition the first dispersant dispersion, wherein P, SVG 15106842.10-24-2016.IUQVGFYLPXXIFW1.CLM.3.12.1462.1188.1596.1208.svg 0.067 0.447 Chemistry Black and white represents the volume of the first acid system, wherein P -r represents the a density of water, and wherein represents the vohume of water; treating the combination liquid with conducting the ultrasonic stirring process on the combined liquid for 0.5-3 hours[[j]] then putting it into conducting a centrifuging centrifugal process on the combined liquid at a rate o f with rotating speed being 4000rm'in for 5min and take the to obtain a supernatant: addi ng an ammonium sulfate solution with a mass concentration of being 2-5% into the supernatant to obtain a third solution and salt it out; salting out the third solution to obtain a fourth solution suction filtrate filtrating the fourth solution and wash the to obtain a filter cake; washing the filter cake with deionized water: alcohol washina the filter cake: and diying the filter cake to obtain the obtaining graphene oxide after a process of alcohol washing and drying.
(Curr ently Am ended) The method of claim 1, wherein said first acid composition in step b compri s eo includes at least one acid selected from the group consisting of concentrated sulfiric acid, fiming sulfuric acid, concentrated nitrite acid nitric acid. fuming nitrite acid nitric acid. perchloric acid, chlorosulfonic acid, trifluoroacetic acid (T FA) and sulphaimic acid: and Page 44 of 49 Application Serial No, 15/406,842 Applicant: SHENZHEAN CANTONE TLENERGY SE RVICES CO- LTD. Art Unit: 1 76 Response to O ffic e Action ma i/ed on 09 SVG 15106842.10-24-2016.IUQVGFYLPXXIFW1.CLM.4.3.1075.354.1121.386.svg 0.107 0.153 Chemistry Black and white 2016 wherein said oxidant in-sep-e oipri e includes at least one oxidant selected fiom the group consisting of nitrate. dichromate., persulphate. permanganate. peroxide, phosphorus oxide, and oxy'iodide.
The method of claim 1, wherein said second acid composition. step e comprises includes at least one agent selected from the group consisting of strong phosphoric acid, pyrophosphoric acid, metaphosphoric acid, glacial acetic acid. propionic acid, adipic acid, and g lutaric acid: and wh ere in said lo ng -chain organi c acid mentioned in step e comprices and at least one agent selected from the group consisting of capric acid, undecylenie acid, lauric acid, tetradecanoic acid, palmitic acid. and octadecanioic acid. i (Cur rently A mended) The method of claim 4, w here in said second acid composition i i n step e comprise; includes at least one agent selected from the group consisting of phosphoric acid, glacial acetic acid, and adipie acid; and wherein said long-chain organic acid in step c comprises includes at least one agent selected from the group consisting of capric acid. palmitic acid, and octadecanioic acid.
(C urr ently Amended) [[A]] The method for preparing graphene of claim 1, further comprising: e. putting adding the graphene oxide obtained according to claim I into a dispersant with a high boiling point, and putting it through conducing an ultrasonic distribution treatment to obtain a j graphene oxide dispersant second dispersion with a concentration of 0.1-1 g/ml: f. putting adding a reducing agent into the second dispersio n; graphene oxide dispersant obtained from ctop e wherein the reducing agent is one of organic acid and organic acid salt, or a mixture of two or more f organic acids and organic acid salts: wherein the a mass ratio of the graphene oxide graphene oxide dispersant to the reducing agent is 1: 2-8; Page 45 of 49 Application Serial No, 15/406,842 Applicant: SHENZHEAN CANTONE TLENERGY SE RVICES CO- LTD. Art Unit: 1 76 Response to Offic e Action mailed on 09 SVG 15106842.10-24-2016.IUQVGFYLPXXIFW1.CLM.5.3.1075.354.1121.386.svg 0.107 0.153 Chemistry Black and white/2016 putting the graphene-ex-ide-depersant with-the-reduemg-agent obtained-rem-sep-f-t-e SVG 15106842.10-24-2016.IUQVGFYLPXXIFW1.CLM.5.4.378.476.400.508.svg 0.107 0.073 Chemistry Black and white conducting a microwave heating process on the second dispersion at of 400-900W for 5-30min; pttA-he-g phenet-eide--ite conducting the ultrasonic stripping process on the second dispersion at 4 100-600W for 0,5-3 hours: and h. add ina water into the second dispersion fifth solutio n-gaphene-e-ie4spersant obtemed in stop g, and wherein a the volume of the water is the same as that of the second dispersion the dispersant: obtaining graphene after filtering suction filtrating. washing, and drying the fifth solution to obtain the graphene composition of water and the graphene oxide dispersant by suction filtrate, and washing and drying.
(C urr ently Am ended) The method of clai m 6, wherein said reducing a g ent in step f comprises i ncludes at least one agent selected from the group consisting of citric acid, gluconic acid, formic acid, ascorbic acid, oxalic acid, sodium citrate, sodimn gluconate, sodium formate, sodium ascorbate, and sodium oxalate.
(C urr ently Amended) The method of claim 9. wherein said reducing agent in step f comprises includes at least one agent selected from the group consisting of oxalic acid, sodium citrate. fonuic acid, and sodium formnate, or a mixture of two or more of them. Page 46 of 49
Materials described outside the worked examples.
crystalline flake graphite
graphene oxide
graphene
ammonium sulfate
(NH₄)2SO₄
first acid composition (strong acid intercalator)
oxidant (nitrate, dichromate, persulphate, permanganate, peroxide, phosphorus oxide, oxyiodide)
first acid composition (concentrated sulfuric acid, fuming nitric acid, perchloric acid, chlorosulfonic acid)
oxidant (nitrate, potassium permanganate, ammonium persulfate, potassium persulfate, nitrite of potash, phosphorus pentoxide, iodine pentoxide)
second acid composition (phosphoric acid, pyrophosphoric acid, metaphosphoric acid, glacial acetic acid, propionic acid, adipic acid, glutaric acid)
long-chain organic acid (capric acid, undecylenic acid, lauric acid, tetradecanoic acid, palmitic acid, octadecanoic acid)
reducing agent (organic acid or organic acid salt)
high boiling point dispersant (phosphoric acid 80%, phosphoric acid 85%, glycerol, glycol, N-methyl-pyrrolidone, triethylene glycol, cyclohexanol)
high boiling point dispersant (phosphoric acid 80%, glycerol, N-methyl-pyrrolidone)
reducing agent (citric acid, gluconic acid, formic acid, ascorbic acid, oxalic acid, sodium citrate, sodium gluconate, sodium formate, sodium ascorbate, sodium oxalate)
reducing agent (oxalic acid, sodium citrate, formic acid, sodium formate)
Additional fabrication and treatment steps described in the patent.
Performance values and ranges asserted in the specification or claims.
| Property | Value | Material |
|---|---|---|
Temperature | ≤ 40 °C | — |
Duration | 0.5–3 hours | — |
Duration | 3–10 min | — |
— | 400–900 W | — |
Duration | 5–30 min | — |
— | 100–600 W | — |
Duration | 5-3 hours | — |
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